CN103449536A - Preparation method of perovskite type nano Nd1-xMgxCoO3 - Google Patents
Preparation method of perovskite type nano Nd1-xMgxCoO3 Download PDFInfo
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- CN103449536A CN103449536A CN2013103871118A CN201310387111A CN103449536A CN 103449536 A CN103449536 A CN 103449536A CN 2013103871118 A CN2013103871118 A CN 2013103871118A CN 201310387111 A CN201310387111 A CN 201310387111A CN 103449536 A CN103449536 A CN 103449536A
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Abstract
The invention relates to a preparation method of a perovskite type material, in particular to a preparation method of perovskite type nano Nd1-xMgxCoO3. The method comprises the following steps: preparing precursor of perovskite type Nd1-xMgxCoO3 by taking Nd2O3, Mg(NO3)2, Co(NO3)3.6H2O, NaOH and Na2CO3 as starting materials by a co-precipitation method; calcining the precursor to obtain the perovskite type nano Nd1-xMgxCoO3. The preparation method has the advantages of readily available raw materials, simpler preparation process, safety, no need of large-sized special equipment, less investment, lower production cost, short production period of products, high efficiency and high purity; the particle diameter of the perovskite type nano Nd1-xMgxCoO3 is mainly distributed between 100 nm and 200 nm; the perovskite type nano Nd1-xMgxCoO3 has better industrial utilization prospect.
Description
Technical field
The present invention relates to a kind of preparation method of Perovskite-type material, be specifically related to a kind of Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method.
Background technology
Perovskite (or uhligite) shaped material belongs to trigonal system, and basic structure is ABO
3, this structure only has positively charged ion on the A ion position (as Ca
2+) onesize or larger than it with oxonium ion, and the B ion is (as Ti
4+) ligancy be to be only stablely at 6 o'clock, the radius between ion meets R
a+ R
o=2
0.5(R
b+ R
o).But, meeting the very considerably less of this ideal situation in real crystal, the crystal of most Perovskite-type structures is not ideal crystal and certain distortion is arranged, the radius between ion meets R
a+ R
o=t2
0.5(R
b+ R
o) (generally t=0.7-1.0).The Perovskite-type material has this special structure just, make the Perovskite-type material there is much special character, as thermoelectricity capability, superconductivity, piezoelectric property, optical property, magnetic performance etc., can improve by doping the performance of Perovskite-type material again in practical application, can say that the Perovskite-type material is a kind of extremely important functional materials, be of wide application, as aspects such as sensor, stopper, light micromotor, memory device, matrix or substrate, catalysis electrode, photoelectric device, gas phase separation film, fuel cells.And nanometer perovskite shaped material has surface effects, small-size effect and the macro quanta tunnel effect of unique nanocrystal and high-density Grain Boundary Character and generation therefrom, make it show the essential distinction of a series of and common polycrystal and non-crystalline solids at aspect of performances such as mechanics, calorifics, magnetics, optics, electricity, acoustics.And adopt cheaply method to prepare nanometer perovskite shaped material, being the key that realizes the nano material widespread adoption, is also current problem demanding prompt solution.
Summary of the invention
The invention provides a kind of co-precipitation-sintering process simple, with low cost and prepare Perovskite-type nanometer Nd
1-xmg
xcoO
3.Described method is simple to operation, needs equipment few, invests littlely, and production cost is low, and efficiency is high, and products obtained therefrom purity is high, has industrial utilization prospect preferably.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, comprise the following steps:
(1) according to Nd
1-xmg
xcoO
3middle metallic element ratio, take the Nd of certain mol proportion
2o
3, Mg (NO
3)
26H
2o and Co (NO
3)
36H
2o; Described x=0 ~ 0.5;
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2the O mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.01~0.05molL
-1solution A; Simultaneously, by Nd
2o
3add a certain amount of dilute nitric acid dissolution, make to obtain Nd
2o
3concentration is 0.01~0.025molL
-1solution B;
(3) A is mixed to also ultrasonic dispersion 10~15min with B, obtain mixed solution A+B;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare respectively 0.2 ~ 0.3 molL after ultrasonic wave is dissolved 10 ~ 15 min
-1naOH solution and 0.2 ~ 0.3 molL
-1na
2cO
3solution, then pour this NaOH solution into Na
2cO
3prepare mixed solution C in solution; Described NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH, Na
2cO
3the two amount of substance and with Co (NO
3)
36H
2the ratio of O amount of substance is 6 ~ 7:1, and standing filtration after ultrasonic 30 ~ 50min, is precipitated sample D;
(6) with distilled water wash sample D, to washings be neutral after suction filtration, then use again the washing with alcohol filter cake, then, by filter cake dry 8~10h under 100 ~ 150 ℃ of conditions, finally dry cake is fully ground to form to the powdery thing, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 1~3 ℃ of min
-1temperature rise rate be heated to 800~900 ℃ the insulation 4.0~6.0h after, natural cooling down, to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, the described certain mol proportion of step (1) is (1-x)/2:x:1.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, the described rare concentration of nitric acid of step (2) is 0.10~0.20molL
-1.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, the described NaOH strength of solution of step (4) is 2.4 molL
-1, described Na
2cO
3strength of solution is 2.4 molL
-1.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, the described presoma powdery of step (6) thing is 200 orders.
According to above-mentioned Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, the described washings neutrality of step (6) is pH6.8~7.0.
positive beneficial effect of the present invention:
The raw materials used wide material sources of the present invention, cheap; The inventive method is simple to operation, safety, and equipment is few, invests littlely, easily produces; Life cycle of the product is short, and efficiency is high, and cost is low, and purity is high, the Perovskite-type nanometer Nd of preparation
1-xmg
xcoO
3particle diameter mainly be distributed between 100~200nm, there is industrial utilization prospect preferably.
The accompanying drawing explanation
The Perovskite-type nanometer Nd that Fig. 1 is the embodiment of the present invention 1 preparation
1-xmg
xcoO
3scanning electron microscope (SEM) picture.
Fig. 2, Fig. 3, Fig. 4 and Fig. 5 are respectively the Perovskite-type nanometer Nd of the embodiment of the present invention 1,2,3,4 preparations
1-xmg
xcoO
3x-ray powder diffraction (XRD) collection of illustrative plates.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment.Test method in following embodiment, if no special instructions, be ordinary method; Test materials and reagent used in following embodiment, if no special instructions, all purchased from conventional chemical reagent shop.
embodiment 1
The present embodiment Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, comprise the following steps:
(1) x=0, according to Nd
1-xmg
xcoO
3the metallic element ratio, take Nd
2o
36.72g(0.02mol) and Co (NO
3)
36H
2o 14.12g(0.04mol);
(2) by Co (NO
3)
36H
2o fully dissolves with 0.8 L distilled water, makes to obtain Co (NO
3)
3concentration is 0.05molL
-1solution A; Simultaneously, by Nd
2o
3add 1L 0.20molL
-1dilute nitric acid dissolution, make to obtain Nd
2o
3concentration is 0.02molL
-1solution B;
(3) A is mixed to also ultrasonic dispersion 10min with B, obtain mixed solution A+B;
(4) by NaOH6.4g(0.16mol) and Na
2cO
38.48g(0.08mol) add respectively in 0.67L and 0.33L distilled water, and prepare respectively 0.24 molL after ultrasonic wave is dissolved 10min
-1naOH solution and 0.24 molL
-1na
2cO
3solution, then pour this NaOH solution into Na
2cO
3prepare mixed solution C in solution;
(5) C is added in A+B, and, after ultrasonic 30min, standing filtration, be precipitated sample D;
(6) with distilled water wash sample D, for neutral (pH is 6.8~7.0) rear suction filtration, then use again the washing with alcohol filter cake to washings, then by filter cake dry 8h under 120 ℃ of conditions, finally dry cake is fully ground to form to 200 order meals, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 3 ℃ of min
-1temperature rise rate be heated to 800 ℃ the insulation 6.0h, natural cooling down, to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3;
Gained Perovskite-type nanometer Nd
1-xmg
xcoO
3(x=0) the very high (see figure 2) of purity, its particle diameter mainly is distributed in (see figure 1) between 140~200nm.
embodiment 2
The present embodiment Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, comprise the following steps:
(1) x=0.5; According to Nd
1-xmg
xcoO
3the metallic element ratio, take Nd
2o
33.36g(0.01mol), Mg (NO
3)
26H
2o 5.12g(0.02mol) and Co (NO
3)
36H
2o 14.12g(0.04mol);
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2the O mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.03molL
-1solution A; Simultaneously, by Nd
2o
3add a certain amount of 0.10molL
-1dilute nitric acid dissolution, make to obtain Nd
2o
3concentration is 0.025molL
-1solution B;
(3) A is mixed to also ultrasonic dispersion 15min with B, obtain mixed solution A+B;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare respectively 0.2 molL after ultrasonic wave is dissolved 15min
-1naOH solution and 0.2molL
-1na
2cO
3solution, then pour this NaOH solution into Na
2cO
3prepare mixed solution C in solution, get NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH and Na
2cO
3with Co (NO
3)
36H
2the mol ratio of O is 7:1, and, after ultrasonic 50min, standing filtration, be precipitated sample D;
(6) with distilled water wash sample D, for neutral (pH is 6.8~7.0) rear suction filtration, then use again the washing with alcohol filter cake to washings, then by filter cake dry 8h under 150 ℃ of conditions, finally dry cake is fully ground to form to 150 order meals, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 1 ℃ of min
-1temperature rise rate be heated to 900 ℃ the insulation 5.0h, natural cooling down, to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3;
Gained Perovskite-type nanometer Nd
1-xmg
xcoO
3(x=0.5) the very high (see figure 3) of purity, its particle diameter mainly is distributed between 130~180nm.
embodiment 3
The present embodiment Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, comprise the following steps:
(1) x=0.2; According to Nd
1-xmg
xcoO
3the metallic element ratio, take Nd
2o
35.38g(0.016mol), Mg (NO
3)
26H
2o 2.05g(0.008mol) and Co (NO
3)
36H
2o 14.12g(0.04mol);
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2the O mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.02molL
-1solution A; Simultaneously, by Nd
2o
3add a certain amount of 0.15molL
-1dilute nitric acid dissolution, make to obtain Nd
2o
3concentration is 0.015molL
-1solution B;
(3) by A and B ultrasonic dispersion 13min, obtain mixed solution A+B;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare respectively 0.3 molL after ultrasonic wave is dissolved 13min
-1naOH and 0.3molL
-1na
2cO
3solution, then pour this NaOH solution into Na
2cO
3prepare mixed solution C in solution, get NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH and Na
2cO
3with Co (NO
3)
36H
2the mol ratio of O is 6:1, and, after ultrasonic 40min, standing filtration, be precipitated sample D;
(6) with distilled water wash sample D, for neutral (pH is 6.8~7.0) rear suction filtration, then use again the washing with alcohol filter cake to washings, then by filter cake dry 10h under 100 ℃ of conditions, finally dry cake is fully ground to form to 250 order meals, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 2 ℃ of min
-1temperature rise rate be heated to 900 ℃ the insulation 4.0h, natural cooling down, to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3;
Gained Perovskite-type nanometer Nd
1-xmg
xcoO
3(x=0.2) the very high (see figure 4) of purity, its particle diameter mainly is distributed between 130~180nm.
embodiment 4
The present embodiment Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, comprise the following steps:
(1) x=0.1; According to Nd
1-xmg
xcoO
3the metallic element ratio, take Nd
2o
36.06g(0.018mol), Mg (NO
3)
26H
2o 1.02g(0.004mol) and Co (NO
3)
36H
2o 14.12g(0.04mol);
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2the O mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.01molL
-1solution A; Simultaneously, by Nd
2o
3add a certain amount of 0.20molL
-1dilute nitric acid dissolution, make to obtain Nd
2o
3concentration is 0.01molL
-1solution B;
(3) A is mixed to also ultrasonic dispersion 12min with B, obtain mixed solution A+B;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare respectively 0.25 molL after ultrasonic wave is dissolved 13min
-1naOH solution and 0.25 molL
-1na
2cO
3solution, then pour this NaOH solution into Na
2cO
3prepare mixed solution C in solution, get NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH and Na
2cO
3with Co (NO
3)
36H
2the mol ratio of O is 7:1, and, after ultrasonic 45min, standing filtration, be precipitated sample D;
(6) with distilled water wash sample D, for neutral (pH is 6.8~7.0) rear suction filtration, then use again the washing with alcohol filter cake to washings, then by filter cake dry 9h under 130 ℃ of conditions, finally dry cake is fully ground to form to 200 order meals, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 2 ℃ of min
-1temperature rise rate be heated to 800 ℃ the insulation 5.0h, natural cooling down, to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3;
Gained Perovskite-type nanometer Nd
1-xmg
xcoO
3(x=0.1) the very high (see figure 5) of purity, its particle diameter mainly is distributed between 100~160nm.
The present invention is not limited to above-mentioned embodiment, and those skilled in the art also can make multiple variation accordingly, but any and the present invention are equal to or similarly change and all should be encompassed in the scope of the claims in the present invention.
Claims (6)
1. a Perovskite-type nanometer Nd
1-xmg
xcoO
3the preparation method, it is characterized in that, comprise the following steps:
(1) according to Nd
1-xmg
xcoO
3middle metallic element ratio, take the Nd of certain mol proportion
2o
3, Mg (NO
3)
26H
2o and Co (NO
3)
36H
2o; Described x=0 ~ 0.5;
(2) by Co (NO
3)
36H
2o and Mg (NO
3)
26H
2the O mixing is fully dissolved with a certain amount of distilled water, makes to obtain Co (NO
3)
3concentration is 0.01~0.05molL
-1solution A; Simultaneously, by Nd
2o
3add a certain amount of dilute nitric acid dissolution, make to obtain Nd
2o
3concentration is 0.01~0.025molL
-1solution B;
(3) A is mixed to also ultrasonic dispersion 10~15min with B, obtain mixed solution A+B;
(4) by a certain amount of NaOH and Na
2cO
3add in distilled water respectively, and prepare respectively 0.2 ~ 0.3 molL after ultrasonic wave is dissolved 10 ~ 15 min
-1naOH solution and 0.2 ~ 0.3 molL
-1na
2cO
3solution, then pour this NaOH solution into Na
2cO
3prepare mixed solution C in solution; Described NaOH and Na
2cO
3mol ratio be 1:0.5;
(5) C is added in A+B, make NaOH, Na
2cO
3the two amount of substance and with Co (NO
3)
36H
2the ratio of O amount of substance is 6 ~ 7:1, and standing filtration after ultrasonic 30 ~ 50min, is precipitated sample D;
(6) with distilled water wash sample D, to washings be neutral after suction filtration, then use again the washing with alcohol filter cake, then, by filter cake dry 8~10h under 100 ~ 150 ℃ of conditions, finally dry cake is fully ground to form to the powdery thing, obtain Nd
1-xmg
xcoO
3presoma;
(7) by Nd
1-xmg
xcoO
3presoma is placed in heating unit, with 1~3 ℃ of min
-1temperature rise rate be heated to 800~900 ℃ the insulation 4.0~6.0h after, natural cooling down, to room temperature, obtains Perovskite-type nanometer Nd
1-xmg
xcoO
3.
2. Perovskite-type nanometer Nd according to claim 1
1-xmg
xcoO
3the preparation method, it is characterized in that: the described certain mol proportion of step (1) is (1-x)/2:x:1.
3. Perovskite-type nanometer Nd according to claim 1
1-xmg
xcoO
3the preparation method, it is characterized in that: the described rare concentration of nitric acid of step (2) is 0.10~0.20molL
-1.
4. Perovskite-type nanometer Nd according to claim 1
1-xmg
xcoO
3the preparation method, it is characterized in that: the described NaOH strength of solution of step (4) is 2.4 molL
-1, described Na
2cO
3strength of solution is 2.4 molL
-1.
5. Perovskite-type nanometer Nd according to claim 1
1-xmg
xcoO
3the preparation method, it is characterized in that: the described presoma powdery of step (6) thing is 200 orders.
6. Perovskite-type nanometer Nd according to claim 1
1-xmg
xcoO
3the preparation method, it is characterized in that: the described washings of step (6) is neutral is pH6.8~7.0.
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Cited By (2)
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CN104628374A (en) * | 2015-01-26 | 2015-05-20 | 华北水利水电大学 | Preparation method of nanometer Nd0.1La0.9FexCo(1-x)O3 material |
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Cited By (2)
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CN104591722A (en) * | 2015-01-05 | 2015-05-06 | 华北水利水电大学 | Perovskite-type nanometer material and preparation method thereof |
CN104628374A (en) * | 2015-01-26 | 2015-05-20 | 华北水利水电大学 | Preparation method of nanometer Nd0.1La0.9FexCo(1-x)O3 material |
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